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Method for preparing methylheptenone

A technology of methyl heptenone and acetone is applied in the field of preparing methyl heptenone by condensation reaction, and can solve the problems of low yield of methyl heptenone and the like

Active Publication Date: 2008-01-16
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for preparing methylheptenone by condensation reaction of chloroisoamylene and acetone generally has a defect, that is, the yield of methylheptenone is low, generally not more than 75%.

Method used

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  • Method for preparing methylheptenone
  • Method for preparing methylheptenone

Examples

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Embodiment 1～6

[0017] In a four-necked flask equipped with a stirring device, a thermometer, a reflux condenser and a balanced dropper, add the catalyst cetyltrimethylammonium bromide according to the required amount, and add the raw material chloroiso pentene and acetone. Start stirring at a stirring speed of 50 r / min, slowly heat to the required reaction temperature, and at the same time quickly dropwise add a pre-prepared sodium hydroxide aqueous solution, the content of sodium hydroxide in the sodium hydroxide aqueous solution is 42-55wt%. When reflux occurs, take out the upper oil phase reaction solution every 10 minutes and filter it with a sand core funnel with a pore size of 15-20 μm to remove the generated sodium chloride, return the filtrate to the original four-necked flask, and repeat this operation until the end of the reaction . After the reaction, all the reaction liquids were taken out and allowed to stand for stratification, and the oil phase was obtained to analyze the com...

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Abstract

The methyl heptenone preparing process adopts chloro isoamyilene and acetone as material and prepares methyl heptenone through condensation inside sodium hydroxide aqua. The present invention has sodium hydroxide aqua concentration of 42-55 wt%, and the molar material ratio of chloro isoamyilene, acetone and sodium hydroxide of 1 to 6.5-8.4 to 7.4-9.6. The catalyst for the condensation is hexadecyl trimethyl ammonium bromide in the amount of 0.2-1.0 wt% of chloro isoamyilene. The reaction at temperature 20-70 deg.c and normal pressure under stirring lasts for 2-6 hr, and the solid sodium chloride grain produced in the reaction is eliminated through filtering. Compared with available technology, the present invention has the advantages of obviously raised methyl heptenone yield of about 80 %.

Description

technical field [0001] The invention relates to a method for preparing methyl heptenone, in particular to a method for preparing methyl heptenone by condensation reaction in aqueous sodium hydroxide solution using chlorinated isopentene and acetone as raw materials. Background technique [0002] Methyl heptenone has a strong chemical reaction ability and can be derived into many kinds of chemical products. It is an important intermediate in the synthesis of medicines, flavors and fragrances. Methyl heptenone is also used to prepare linalool, citral and pseudoionone The main raw material, which can further prepare vitamin A, vitamin E, vitamin K1 and various spices and flavors. [0003] The isoprene method is one of the main process routes for producing methylheptenone. The isoprene is first reacted with hydrogen chloride to generate chlorinated isopentene, and then the chlorinated isopentene is reacted with acetone in the presence of lye. The condensation reaction produces ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/203C07C45/68
Inventor 郭世卓杨忠保李伟祁正娟周秀凤
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD